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A snapshot of high-entropy alloy processing techniques and their effects on resulting mechanical properties

High-entropy alloys (HEAs) exhibit exceptional strength, corrosion resistance, and thermal stability, making them promising candidates for nuclear, aerospace, and other extreme applications. While most prior work has focused on compositional design, manufacturing techniques themselves can alter microstructure and mechanical properties as dramatically as alloy chemistry. This review compiles and compares the effects of processing routes—including arc melting, induction melting, mechanical alloying with spark plasma sintering, and additive manufacturing—on the structure and properties of HEAs. Quantitative comparisons highlight, for example, that SPS-processed alloys can achieve ∼20–45 % higher yield and tensile strength than arc-melted counterparts, while Bridgman solidification produces nearly single-crystal structures with elongation to failure exceeding 80 %. Additive manufacturing routes such as selective laser melting offer fine microstructures but also introduce anisotropy and porosity, leading to yield strengths spanning 100–600 MPa for the same composition. By synthesizing such results, this review provides actionable insight into how processing routes interact with HEA core effects (high entropy, lattice distortion, sluggish diffusion, and cocktail effect) to determine performance, thereby offering a practical guide for optimizing manufacturing strategies.

36 MATERIALS SCIENCE↗

Manufacturing Oxide Dispersion Strengthened (ODS) steel plate via cold spray and friction stir processing

Oxide dispersion strengthened (ODS) steels, traditionally fabricated by ball milling and conventional powder metallurgy techniques to achieve bulk form, followed by intricate rolling and thermal treatment steps to achieve plate or sheet form. Here, we present a novel processing route that combines cold spray (CS) with friction stir processing (FSP) to manufacture ODS steel plate directly from gas atomization reaction synthesis (GARS)-prepared powder, thus no rolling steps involved. Microstructural and mechanical characterizations were performed to assess the quality and properties of the resulting ODS steel plate. Our findings demonstrate that the slightly porous CS deposited layer was fully consolidated after FSP, yielding a fully dense ODS steel plate that exhibited a favorable tradeoff between strength and ductility upon extraction from the substrate. Furthermore, through microstructural analysis, we revealed the presence of an appreciable density (∼10 22 /m 3 ) of nano-sized oxide particles, with the majority being smaller than 5 nm via the combined CS + FSP fabrication route. This work serves as a first proof-of-concept demonstration of the manufacturing approach described herein, offering a possible alternative route for producing ODS steel plates.

36 MATERIALS SCIENCE↗

Effect of solvents on morphologies of PbTe nanostructures: Controllable synthesis of hollow and solid PbTe nanocubes by a solvothermal method

We demonstrate a facile solvothermal route to grow hollow and solid PbTe nanocubes. The hollow PbTe nanocubes were successfully achieved when EtOH was used as solvent in the presence of nonionic polymer PEG, while the solid PbTe nanocubes were obtained when EG was used as solvent in the presence of PEG, whilst keeping the other experimental conditions constant. The results indicate that the solvents used in reaction system play a key role to determine the interior structure of PbTe nanocubes. On the basis of the experimental results and analysis, a possible growth mechanism has been discussed in detail for the hollow and solid PbTe nanocubes. - Graphical abstract: A facile solution-phase route has been developed to synthesize hollow and solid PbTe nanocubes. The possible growth mechanism of hollow and solid PbTe nanocubes was discussed in detail. Highlights: Black-Right-Pointing-Pointer A facile controllable route was described for hollow and solid PbTe nanocubes. Black-Right-Pointing-Pointer The hollow PbTe nanocubes were achieved using EtOH as solvent. Black-Right-Pointing-Pointer The solid PbTe nanocubes were obtained using EG as solvent. Black-Right-Pointing-Pointer The solvent played a key role for the formation of hollow and solid PbTe nanocubes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Synthesis of manganese spinel nanoparticles at room temperature by coprecipitation

This paper is focused on a new route to synthesize Mn{sub 3}O{sub 4} nanoparticles by alkalisation by sodium hydroxide on a manganeous solution at room temperature. The precipitates obtained at different pH values have been characterized by XRD and TEM. Since the first addition of sodium hydroxide, a white Mn(OH){sub 2} precipitate appears. At pH=7, {gamma}-MnOOH phase is predominant with needle like shaped particles. At pH=10, hausmanite nanoparticles, which exhibits well defined cubic shape in the range 50-120 nm are obtained. This new precipitation route is a fast and easy environmentally friendly process to obtain well crystallized hausmanite nanoparticles. - Graphical abstract: TEM image showing Mn{sub 3}O{sub 4} particles after a precipitation at pH=10. Highlights: Black-Right-Pointing-Pointer A new route to synthesize Mn{sub 3}O{sub 4} nanoparticles has been demonstrated. Black-Right-Pointing-Pointer Synthesis has been performed by precipitation at room temperature. Black-Right-Pointing-Pointer The size of the Mn{sub 3}O{sub 4} nanoparticles is between 50 and 120 nm.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Synthesis dependent characteristics of Sr{sub 1-x}Mn{sub x}TiO{sub 3} (x=0.03, 0.05, 0.07 and 0.09)

Sr{sub 1-x}Mn{sub x}TiO{sub 3} (where x=0.03, 0.05, 0.07 and 0.09) was synthesized via different routes that include solid-state, oxalate precipitation and freeze drying. In oxalate precipitation technique, compositions corresponding to 3 and 5 mol% doping of Mn were monophasic whereas the higher compositions revealed the presence of the secondary phases such as MnO, Mn{sub 3}O{sub 4} etc., as confirmed by high resolution X-ray diffraction (XRD) studies. The decomposition behavior of the precursors prepared using oxalate precipitation method corresponding to the above mentioned compositions was studied. Nanopowders of compositions pertaining to 5 to 9 mol% of Mn doping were obtained using freeze-drying technique. The average crystallite size of these nanopowders was found to be in the 35 to 65 nm range. The microstructural studies carried out on the sintered ceramics, fabricated using powders synthesized by different routes established the fine grained nature (<1 {mu}m) of the one obtained by freeze drying method. Raman scattering studies were carried out in order to complement the observations made from XRD regarding the phase purity. The dielectric properties of the ceramics obtained by different synthesis routes were studied in the 80-300 K temperature range at 100 kHz and the effect of grain size has been discussed. - Graphical abstract: XRD patterns of Sr{sub 1-x}Mn{sub x}TiO{sub 3} (x=0.03 and 0.05) obtained by oxalate precipitation technique along with that of the nanopowders for x=0.05, 0.07 and 0.09 obtained by freeze drying method, microstructural characterization and synthesis dependent dielectric behavior. Highlights: Black-Right-Pointing-Pointer Monophasic samples obtained for compositions Sr{sub 1-x}Mn{sub x}TiO{sub 3} with x=0.03 and 0.05. Black-Right-Pointing-Pointer Nanopowders of Sr{sub 1-x}Mn{sub x}TiO{sub 3} with x=0.05, 0.07 and 0.09 were synthesized by freeze-drying method. Black-Right-Pointing-Pointer Phase purity of samples synthesized using freeze drying method were studied at different sintering temperatures. Black-Right-Pointing-Pointer Analysis of Raman spectra for samples prepared by both oxalate precipitation and freeze-drying. Black-Right-Pointing-Pointer Microstructure dependent dielectric characteristics have been illustrated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

From fluorite to pyrochlore: Characterisation of local and average structure of neodymium zirconate, Nd{sub 2}Zr{sub 2}O{sub 7}

The structural characterisation of Nd{sub 2}Zr{sub 2}O{sub 7} prepared via a precursor route was performed using a combination of local and average structure probes (neutron total scattering, X-ray and neutron diffraction). We present the first total scattering and reverse Monte Carlo (RMC) modelling study of Nd{sub 2}Zr{sub 2}O{sub 7}, which provides compelling evidence for the adoption of a disordered fluorite-type structure by Nd{sub 2}Zr{sub 2}O{sub 7} prepared by a low-temperature precursor route. Annealing the material at high temperatures leads to a transformation to a pyrochlore-type structure; however, Rietveld refinement using powder neutron diffraction data shows that the oxygen sublattice retains a degree of disorder. - Graphical abstract: Display Omitted - Highlights: • The first total scattering and RMC modelling study of Nd{sub 2}Zr{sub 2}O{sub 7}. • Demonstration that the synthetic route influences the crystal structure adopted. • Insight into the importance of total scattering in studies of complex superstructures, especially for nano-sized materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Synthesis and characterization of novel barium iron phosphates: Insight into new structure types tailored by hydrogen atoms

A significant gap in our knowledge of phosphate crystal chemistry is the lack of understanding of what controls the depolymerization of [PO{sub 4}] tetrahedra. A new route using phosphoric acid without any added water at 240 °C has been developed to synthesize two new compounds Ba{sub 2}Fe{sub 2}[H(PO{sub 3}OH){sub 2}][H(P{sub 2}O{sub 7}){sub 2}] and Ba{sub 2}Fe[H(P{sub 2}O{sub 7}){sub 2}], as well as a new polymorph β-BaFe{sub 2}(P{sub 2}O{sub 7}){sub 2} from annealing the former at ≥500 °C. Structural characterizations show that Ba{sub 2}Fe{sub 2}[H(PO{sub 3}OH){sub 2}][H(P{sub 2}O{sub 7}){sub 2}] features a novel 2D {sup 2}{sub ∞}([Fe{sub 2}[H(PO{sub 3}OH){sub 2}][H(P{sub 2}O{sub 7}){sub 2}]]{sup 4−}) layer structure containing both hydrogen-diphosphate [H(P{sub 2}O{sub 7}){sub 2}] and hydrogen-monophosphate [H(PO{sub 3}OH){sub 2}] groups, whereas Ba{sub 2}Fe[H(P{sub 2}O{sub 7}){sub 2}] and β-BaFe{sub 2}(P{sub 2}O{sub 7}){sub 2} possess an 1D chain structure and a 3D framework structure, respectively. These structures support a control of hydrogen on the depolymerization of [PO{sub 4}] groups and our work opens a new way for the synthesis of other novel phosphates using controlled water activities. - Graphical abstract: A new route of controlled water activities led to syntheses of three new compounds, indicating water plays a crucial role in the formation of novel phosphates. - Highlights: • A new mild thermal route for the synthesis of novel phosphates. • Water activities controlling the reaction: 2H{sub 3}PO{sub 4}↔H{sub 4}P{sub 2}O{sub 7}+H{sub 2}O. • Phosphate with mixed hydrogen-monophosphate and diphosphate groups. • H atoms in the structural backbone affect the depolymerization of PO{sub 4} groups.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Understanding the infrared to visible upconversion luminescence properties of Er{sup 3+}/Yb{sup 3+} co-doped BaMoO{sub 4} nanocrystals

In this paper we report the infrared to visible upconversion luminescence properties of Er{sup 3+}/Yb{sup 3+} co-doped BaMoO{sub 4} nanocrystals synthesized via microwave assisted sol–gel processing route. Structural, morphological and upconversion luminescence properties were investigated by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), UV–vis diffuse reflectance spectroscopy (UV–vis DRS) and Upconversion Photoluminescence spectra analysis. Results revealed that the oval shaped BaMoO{sub 4} nanocrystals ranging in size from 40 to 60 nm having tetragonal scheelite crystal structure were obtained by sol–gel route. The infrared to visible upconversion luminescence has been investigated in Er{sup 3+}/Yb{sup 3+} co-doped in BaMoO{sub 4}with different Yb{sup 3+} concentrations. Intense green upconversion emissions around 528, 550 nm, and red emission at 657 nm corresponding to the {sup 2}H{sub 11/2}, {sup 4}S{sub 3/2}, and {sup 4}F{sub 9/2} transitions, respectively to the {sup 4}I{sub 15/2} ground state were observed when excited by CW laser radiation at 980 nm. The green emissions were greatly enhanced after the addition of sensitizer (Yb{sup 3+} ions). The effect of Yb{sup 3+} on the upconversion luminescence intensity was analyzed and explained in terms of the energy transfer process based. The reported work establishes the understanding of molybdates as an alternative host material for upconversion luminescence. - Graphical abstract: Infrared to visible upconversion luminescence of Er{sup 3+}/Yb{sup 3+} co-doped BaMoO{sub 4} nanocrystals. - Highlights: • Nanocrystals were synthesized by microwave assisted sol–gel processing route. • Strong green emissions were observed in Er{sup 3+}/Yb{sup 3+} co-doped BaMoO{sub 4} nanocrystals. • Provides an insight on Upconversion luminescence properties of oxides host materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Perovskite LaPbMSbO{sub 6} (M=Co, Ni): Structural distortion, magnetic and dielectric properties

The B-site ordered double perovskite oxides LaPbMSbO{sub 6} (M=Co, Ni) have been synthesized via the modified Sol–Gel precursor two-step route. Rietveld refinements reveal strong abnormal structural distortion and BO{sub 6} octahedral deformation appearing along the ab plane. Owing to the cooperative Jahn–Teller effect of Co{sup 2+} and Pb{sup 2+} ions, the Co-related compound exhibits almost complete Co{sup 2+}–Sb{sup 5+} order. For magnetic properties, spin-canted antiferromagnetic state with high extent of magnetic frustration is confirmed. The Ni-related compound presents heavier magnetic frustration for introducing tiny disorder on site occupation accompanied with valence state and further enhancing the complexity of magnetic competition. Dielectric measurements present a considerable temperature dependent dielectric relaxation with great dc-like loss feature in the LaPbCoSbO{sub 6}. For LaPbNiSbO{sub 6}, however, the permittivity with low dielectric loss is shown to be insensitive to either temperature or frequency. The corresponding electronic active energy manifests that the weakly bounded 3d-electron is prone to hop in a more distorted Co–Sb sublattice. - Graphical abstract: XRD Rietveld refinement result of LaPbCoSbO{sub 6} presented a large BO{sub 6} octahedral distortion along the ab plane. Based upon the variations from Co–O–Sb bond angles, a fierce competition from many extended magnetic coupling routes (M–O–O–M) would induce a considerably large magnetic frustration and electron hopping restriction. - Highlights: • Highly ordered LaPbMSbO{sub 6} (M=Co, Ni) were synthesized. • Abnormal structural distortion appeared in the ab plane. • Strong magnetic frustration was confirmed via M{sup 2+}–O–O–M{sup 2+} route. • Dielectric measurements presented a large difference between Co and Ni samples. • 3d-electronic structure determines lattice distortion and physical properties.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

LiBi{sub 3}S{sub 5}—A lithium bismuth sulfide with strong cation disorder

Among chalcogenide semiconductors for thermoelectric applications, alkali-metal bismuth compounds occur in many complex compositions favorable for high performance. Although LiBi{sub 3}S{sub 5} had been announced in 1977, the potential 1D lithium-ion conductor has hitherto eluded selective synthesis and structure determination. In this study, we present a solid-state route to phase-pure LiBi{sub 3}S{sub 5} powder starting from LiBiS{sub 2} and Bi{sub 2}S{sub 3}. Neutron diffractograms and lithium NMR spectra reveal its crystal structure to be a cation-disordered variety of the AgBi{sub 3}S{sub 5} type (synthetic pavonite; monoclinic, C2/m). Topological analyses and lithium NMR relaxometry suggest that correlated lithium-ion diffusion with activation energies up to 0.66(2) eV occurs along the channels in b direction including tetrahedral voids. Because of cation disorder, immobile bismuth(III) ions clog these pathways, making LiBi{sub 3}S{sub 5} a moderate to poor ionic conductor. The synthesis route reported is nonetheless promising for new lithium bismuth sulfides with, possibly ordered, structure types of the pavonite homologous series. - Graphical abstract: Phase-pure LiBi{sub 3}S{sub 5} has been synthesized and shown to crystallize in cation-disordered variety of the AgBi{sub 3}S{sub 5} type (synthetic pavonite, C2/m) using neutron diffractometry. Topological analyses and NMR relaxometry suggest that immobile Bi{sup 3+} ions clog migration channels along b, making the material a poor lithium conductor. Display Omitted - Highlights: • Phase-pure LiBi{sub 3}S{sub 5} has been synthesized using a promising solid-state route. • LiBi{sub 3}S{sub 5} crystallizes in a cation-disordered variant of the AgBi{sub 3}S{sub 5} type. • Topological analyses suggest lithium diffusion in channels along b. • NMR relaxometry finds activation energies of diffusion as high as 0.66(2) eV. • Because of disorder, LiBi{sub 3}S{sub 5} is a moderate to poor lithium-ion conductor.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Heterometallic metal-organic framework-templated synthesis of porous Co{sub 3}O{sub 4}/ZnO nanocage catalysts for the carbonylation of glycerol

The efficient synthesis of glycerol carbonate (GLC) has recently received great attention due to its significance in reducing excess glycerol in biodiesel production as well as its promising applications in several industrial fields. However, the achievement of high conversion and high selectivity of GLC from glycerol in heterogeneous catalytic processes remains a challenge due to the absence of high-performance solid catalysts. Herein, highly porous nanocage catalysts composed of well-mixed Co{sub 3}O{sub 4} and ZnO nanocrystals were successfully fabricated via a facile heterometallic metal-organic framework (MOF)-templated synthetic route. Benefiting from a high porosity and the synergistic effect between Co{sub 3}O{sub 4} and ZnO, the as-prepared composite catalysts exhibited a significantly enhanced production efficiency of GLC in the carbonylation reaction of glycerol with urea compared to the single-component counterparts. The yield of GLC over the Co{sub 50}Zn{sub 50}-350 catalyst reached 85.2%, with 93.3% conversion and near 91% GLC selectivity, and this catalytic performance was superior to that over most heterogeneous catalysts. More importantly, the proposed templated synthetic strategy of heterometallic MOFs facilitates the regulation of catalyst composition and surface structure and can therefore be potentially extended in the tailoring of other metal oxide composite catalysts. - Graphical abstract: Highly porous Co{sub 3}O{sub 4}/ZnO nanocages were fabricated via a heterometallic MOF-templated route and exhibited a significantly enhanced photocatalytic performance in the production of glycerol carbonate. Display Omitted - Highlights: • Porous Co{sub 3}O{sub 4}/ZnO nanocages were synthesized by a facile thermolysis route of heterometallic MOFs. • The as-prepared nanocages possessed massive pores and Co{sub 3}O{sub 4}/ZnO heterojunctions. • The Co{sub 3}O{sub 4}/ZnO ratio in the composites was easily adjusted by tuning the Co/Zn ratio in the precursors. • The composite catalysts exhibited a significantly enhanced production efficiency of glycerol carbonate in the carbonylation reaction of glycerol with urea.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Characterization of Cu{sub 6}Sn{sub 5} intermetallic powders produced by water atomization and powder heat treatment

Since the Cu{sub 6}Sn{sub 5} intermetallic shows its importance in industrial applications, the Cu{sub 6}Sn{sub 5} intermetallic-containing powders, produced by a powder processing route with a high production rate, were characterized. The route consisted of water atomization of an alloy melt (Cu–61 wt.% Sn) and subsequent heat treatment of the water-atomized powders. Characterization of the water-atomized powders and their heated forms was conducted by using X-ray diffraction, scanning electron microscopy and transmission electron microscopy. Fine water-atomized powder microstructures consisted of primary hexagonal η-Cu{sub 6.25}Sn{sub 5} dendrites coexisting with interdendritic η-Cu{sub 6.25}Sn{sub 5} + β-Sn eutectic. Solidification of fine melt droplets was governed by surface nucleation and growth of the primary hexagonal η-Cu{sub 6.25}Sn{sub 5} dendrites followed by η-Cu{sub 6.25}Sn{sub 5} + β-Sn eutectic solidification of the remnant liquid. In coarse melt droplets, nucleation and growth of primary ε-Cu{sub 3}Sn dendrites were followed by peritectic reaction (ε-Cu{sub 3}Sn + liquid → η-Cu{sub 6.25}Sn{sub 5}) or direct crystallization of η-Cu{sub 6.25}Sn{sub 5} phase from the undercooled melt. Finally, the η-Cu{sub 6.25}Sn{sub 5} + β-Sn eutectic solidification of the remnant liquid occurred. Heating of the water-atomized powders at different temperatures resulted in microstructural homogenization. The water-atomized powders with mixed phases were transformed to powders with single monoclinic ή-Cu{sub 6}Sn{sub 5} phase. - Highlights: • The Cu{sub 6}Sn{sub 5} intermetallic powder production route was proposed. • Single phase Cu{sub 6}Sn{sub 5} powders could be by water atomization and heating. • Water-atomized Cu–Sn powders contained mixed Cu–Sn phases. • Solidification and heat treatment of water-atomized Cu–Sn powders are explained.

36 MATERIALS SCIENCE↗

Layered-structural monoclinic–orthorhombic perovskite La{sub 2}Ti{sub 2}O{sub 7} to orthorhombic LaTiO{sub 3} phase transition and their microstructure characterization

The layered-structural ceramics, such as lanthanum titanate (La{sub 2}Ti{sub 2}O{sub 7}), have been known for their good temperature and low dielectric loss at microwave frequencies that make them good candidate materials for high frequency applications. However, few studies have been conducted on the synthesis optimization by sol gel reaction, in particular by acrylamide polymerization route. The interest in La{sub 2}Ti{sub 2}O{sub 7} ceramic has been greatly increased recently due to the effect of oriented grains. This anisotropy of the microstructure leads to anisotropy in dielectric, electrical and mechanical properties. In this study, grain oriented lanthanum titanate was produced by the sol–gel acrylamide polymerization route. The characterizations of the samples were achieved by thermal analysis, X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), and transmission electron microscopy (TEM). X-ray diffraction indicates that the formation of monoclinic perovskite La{sub 2}Ti{sub 2}O{sub 7} nanocrystals is a necessary first step to obtain orthorhombic LaTiO{sub 3} nanocomposites (with space group Pbnm). In this work we identified that the monoclinic perovskite La{sub 2}Ti{sub 2}O{sub 7} with space group P2{sub 1} transforms its structure into one with the orthorhombic space group Cmc2{sub 1} at approximately 1073 K. The microstructure associated consisted of flaky monoclinic La{sub 2}Ti{sub 2}O{sub 7} nanocomposites in comparison with round-shaped LaTiO{sub 3} nanocomposites. - Highlights: • The flaky-like La{sub 2}Ti{sub 2}O{sub 7} compound was synthesized by sol–gel acrylamide route. • Simultaneous monitoring of the DTA and XRD with temperature was performed. • Phase transformation characterization of La{sub 2}Ti{sub 2}O{sub 7} has been carried out. • The variation of the La{sub 2}Ti{sub 2}O{sub 7} and LaTiO{sub 3} grain morphology has been compared.

36 MATERIALS SCIENCE↗

Facile synthesis and characterization of erythrocyte-like Y-doped PbWO{sub 4} mesocrystals and their photocatalytic activity

Novel erythrocyte-like Y-doped PbWO{sub 4} mesocrystals with average diameter and thickness of 1.5 and 0.7 μm are fabricated via a facile co-precipitation route at room temperature in the ethylene glycol (EG)-water mixed solvent. Time-dependent samples centrifuged at different times are carefully characterized by powder X-ray diffraction (pXRD), field-emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HRTEM) and Raman spectrum. The possible formation mechanism for the novel erythrocyte-like mesocrystals is proposed on the basis of these observations. The photocatalytic activity of the Y-doped PbWO{sub 4} mesocrystals is further investigated in terms of the degradation of the acid orange II under UV irradiation. This simple and environment-friendly strategy presented here offers promising route for the synthesis of other inorganic materials with unique morphologies and interesting properties. - Graphical abstract: Display Omitted - Highlights: • Novel erythrocyte-like Y-doped PbWO{sub 4} mesocrystals are firstly synthesized via a facile co-precipitation route. • The mesocrystals are assembled by small nanoparticles a common crystallographic fashion. • The erythrocyte-like mesocrystals exhibit well photocatalytic activity. • A recrystallization-growth-oriented attachment formation mechanism is proposed.

36 MATERIALS SCIENCE↗

Evolution of carbides in cold-work tool steels

This study aimed to present the complete history of carbide evolution in a cold-work tool steel along its full processing route for fabrication and application. A sequence of processes from cast to final hardening heat treatment was conducted on an 8% Cr-steel to reproduce a typical commercial processing route in a small scale. The carbides found at each process step were then identified by electron diffraction with energy dispersive spectroscopy in a scanning or transmission electron microscope. After solidification, MC, M{sub 7}C{sub 3} and M{sub 2}C carbides were identified and the last one dissolved during hot compression at 1180 °C. In a subsequent annealing at 870 °C followed by slow cooling, M{sub 6}C and M{sub 23}C{sub 6} were added, while they were dissolved in the following austenitization at 1030 °C. After the final tempering at 520 °C, fine M{sub 23}C{sub 6} precipitated again, thus the final microstructure was the tempered martensite with MC, M{sub 7}C{sub 3} and M{sub 23}C{sub 6} carbide. The transient M{sub 2}C and M{sub 6}C originated from the segregation of Mo and finally disappeared due to attenuated segregation and the consequent thermodynamic instability. - Highlights: • The full processing route of a cold-work tool steel was simulated in a small scale. • The carbides in the tool steel were identified by chemical–crystallographic analyses. • MC, M{sub 7}C{sub 3}, M{sub 2}C, M{sub 6}C and M{sub 23}C{sub 6} carbides were found during the processing of the steel. • M{sub 2}C and M{sub 6}C finally disappeared due to thermodynamic instability.

36 MATERIALS SCIENCE↗

Synthesis of Sn-doped ZnO nanorods and their photocatalytic properties

Graphical abstract: Sn-doped ZnO nanorods have been fabricated by a hydrothermal route. Photocatalytic activity of the Sn-doped ZnO samples increases gradually with an increase of the Sn content. Highlights: {yields} Sn-doped ZnO nanorods were fabricated by a hydrothermal route. {yields} Solid-state NMR result confirms Sn{sup 4+} was incorporated into the lattice of ZnO. {yields} The visible luminescence intensity increased with increase in Sn concentration. {yields} Photocatalytic activity of Sn-doped ZnO increases with increasing Sn content. -- Abstract: Sn-doped ZnO nanorods were fabricated by a hydrothermal route, and characterized by X-ray diffraction, field emission scanning electron microscope, UV-vis spectroscopy, Raman spectra, solid-state nuclear magnetic resonance (NMR) spectra, and room temperature photoluminescence spectroscopy. Solid-state NMR result confirms that Sn{sup 4+} was successfully incorporated into the crystal lattice of ZnO. Room temperature photoluminescence showed that all the as-synthesized products exhibited a weak UV emission (380 nm) and a strong visible emission (540 nm), but the intensities of the latter emission increased with increase in Sn concentration. The improvement of visible emission at 540 nm in the Sn-doped ZnO samples was suggested to be a result of the lattice defects increased by doping of Sn in zinc oxide. In addition, the photocatalytic studies indicated that Sn-doped ZnO nanorods are a kind of promising photocatalyst in remediation of water polluted by some chemically stable azo dyes.

36 MATERIALS SCIENCE↗

One-pot synthesis of CuFeSe{sub 2} cuboid nanoparticles

Graphical abstract: CuFeSe{sub 2} cuboid nanoparticles with a tetragonal phase have been successfully synthesized via chemical route from a nonaqueous solution of octadecylamine solvent and metal chloride of precursor. Highlights: {yields} CuFeSe{sub 2} cuboid nanoparticles were prepared by a cost-effective and simple one-pot chemical route. {yields} Synthesized temperature and octadecylamine solvent play a significant role in the cuboid shape of nanoparticles. {yields} The nanocrystallinity feature and tetragonal phase of the CuFeSe{sub 2} nanoparticles were confirmed by HRTEM. -- Abstract: Ternary semiconducting CuFeSe{sub 2} nanocrystals of a particular shape and size were successfully synthesized using a cost-effective and simple one-pot chemical route. X-ray powder diffraction and field emission scanning electron microscopy results indicated that the as-synthesized CuFeSe{sub 2} comprised cuboid nanoparticles with dimensions of 50-150 nm as well as a tetragonal phase. Elemental analysis yielded an atomic ratio of Cu:Fe:Se of 1:1.06:2.17. The synthesis temperature and the solvent octadecylamine were significant in determining the structural phases and morphologies of the final products. The optimal condition for synthesizing the tetragonal CuFeSe{sub 2} phase with cuboid nanoparticles was a reaction temperature of 200 {sup o}C for 1 h in octadecylamine solvent. A possible mechanism of the formation of ternary CuFeSe{sub 2} nanoparticles with controllable shapes is discussed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High rate performances of the cathode material LiNi{sub 1/3}Co{sub 1/3}Mn{sub 1/3}O{sub 2} synthesized using low temperature hydroxide precipitation

Graphical abstract: A low-temperature reaction route is introduced based on hydroxide precipitation method to synthesize a cathode material LiNi{sub 1/3}Co{sub 1/3}Mn{sub 1/3}O{sub 2}. The charge-discharge tests were performed at 1000 mA g{sup -1} between 2.5 and 4.5 V and the discharge capacity is about 160 mAh g{sup -1}. The discharge capacity of the material is strongly impacted by the reaction temperature. The powders sintered at 850 {sup o}C show the best electrochemical performance. Highlights: {yields} A low-temperature reaction route is introduced based on hydroxide precipitation method to synthesize a novel cathode material LiNi{sub 1/3}Co{sub 1/3}Mn{sub 1/3}O{sub 2}. {yields} The charge-discharge tests were performed at higher current as 5 C between 2.5 and 4.5 V. {yields} The discharge capacity of the material is strongly impacted by the reaction temperature. The powders sintered at 850 {sup o}C show the best electrochemical performance. -- Abstract: A low-temperature reaction route is introduced based on hydroxide precipitation method to synthesize the cathode material LiNi{sub 1/3}Co{sub 1/3}Mn{sub 1/3}O{sub 2}. The crystal structure and morphology of the prepared powder have been characterized by X-ray diffraction and Scan electron microscope, respectively. The charge-discharge tests were performed between 2.5 and 4.5 V. The discharge capacity of the material is strongly impacted by the reaction temperature. The powders sintered at 850 {sup o}C show the best electrochemical performance and the initial discharge capacity is about 160 mAh g{sup -1} at 5 C. Powder X-ray diffraction and Scan electron microscope results reveal that the excellent electrochemical performances should be ascribed to the lower precursor reaction temperature, the lower degree of cation mixing and analogous spherical small particles, which can improve the transfer of Li ions and electrons. All these results indicate that this material has potential application in lithium-ion batteries.

36 MATERIALS SCIENCE↗